HRID274046

反应详情

EQUATION

反应方程式

HRID 274046 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of 8-benzylamino-6,7,8,9-tetrahydro-5H-benzocyclohepten-2-ol (970 mg) and 1,1,1-trichloro-2-methyl-2-propanol hydrate (1.28 g) in acetone (30 ml) was added portionwise powder KOH (1.71 g) and the mixture was stirred for 20 hours at ambient temperature. After the solvent was evaporated in vacuo, the residue was poured into 1N sodium hydroxide (30 ml) and washed with diethyl ether. The pH of the aqueous layer was adjusted to 6.0 with 3N hydrochloric acid. The precipitates were filtered off. The filtrate was concentrated in vacuo and water was added to the residue. The resulting precipitates were collected by filtration and dried to give 2-[8-benzylamino-6,7,8,9-tetrahydro-5H-benzocyclohepten-2-yloxy]-2-methylpropionic acid (0.51 g).

WORKUP

后处理

  1. customAfter the solvent was evaporated in vacuo
  2. additionthe residue was poured into 1N sodium hydroxide (30 ml)
  3. washwashed with diethyl ether
  4. filtrationThe precipitates were filtered off
  5. concentrationThe filtrate was concentrated in vacuo and water
  6. additionwas added to the residue
  7. customThe resulting precipitates
  8. filtrationwere collected by filtration
  9. customdried